CN109338421A - A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment - Google Patents

A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment Download PDF

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CN109338421A
CN109338421A CN201811521153.5A CN201811521153A CN109338421A CN 109338421 A CN109338421 A CN 109338421A CN 201811521153 A CN201811521153 A CN 201811521153A CN 109338421 A CN109338421 A CN 109338421A
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copper
plating
cyanide
activation
high temperature
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CN109338421B (en
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王鸥
贾亚洲
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China Hangfa Guizhou Red Forest Air Power Control Technology Co Ltd
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China Hangfa Guizhou Red Forest Air Power Control Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19—Iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The present invention provides a kind of cyanide-free copper electroplating techniques of high temperature resistant thermo-chemical treatment, it is characterised in that: including non-cyanide pre-plating copper pre-treatment, activation protection, non-cyanide pre-plating copper, no cyanogen thickening copper facing pre-treatment, no cyanogen thickening copper facing.This electroplating technology enhances plating solution complexing power based on the displacement copper solved the problems, such as in electroplating process, inhibits the displacement copper phenomenon in electroplating process；Reinforce electroplating work procedure control simultaneously, keep part surface active state before plating, improve binding force of cladding material comprehensively, so that coating is met heat-resisting high-temperature process for a long time, play antiseepage copper facing protective effect.

Description

A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment
Technical field
The present invention relates to a kind of cyanide-free copper electroplating technique, especially a kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment.
Background technique
Since copper plate crystallization is careful, porosity is low, is commonly used for antiseepage protective coating in steel part in heat treatment process, i.e., First part entirety copper facing；Secondly high temeperature chemistry heat treatment need to being carried out using the removing of machine adding method, (such as carburizing, seeps cyanogen at nitriding Deng) the local surfaces layers of copper of part, then one-piece parts carry out high temeperature chemistry heat treatment, finally remove the copper facing in non-antiseepage face Layer.Therefore such copper plate requires have sufficiently strong binding force, is resistant to long heat treatment high temperature, can sufficiently stop carburizing, seep Nitrogen, infiltration cyanogen etc..
Traditional cyanide copper plating process, cyanogen root complex copper ion is very capable, and it is existing that displacement copper seldom occurs in electroplating process As binding force of cladding material is strong, is resistant to high temeperature chemistry heat treatment, but it belongs to backward, severe toxicity, high pollution industry, country and local government Superseded electroplating technology is prohibited always；Due to using non-cyanide ion complex copper, complexing power declines for cyanide-free copper electroplating plating, Displacement copper phenomenon easily occurs in electroplating process, displaced copper at powdered, be easily adsorbed on workpiece in tank liquor and cause coating Binding force decline, it is difficult to bear long heat treatment high temperature, foaming phenomena often occurs after high temperature in coating, is unable to reach antiseepage guarantor The purpose of shield.
Summary of the invention
The object of the present invention is to provide a kind of cyanide-free copper electroplating techniques of high temperature resistant thermo-chemical treatment.This electroplating technology is vertical It is enough to solve the problems, such as the displacement copper in electroplating process, enhances plating solution complexing power, inhibit the displacement copper phenomenon in electroplating process；Together The control of Shi Jiaqiang electroplating work procedure keeps part surface active state before plating, binding force of cladding material is improved comprehensively, when coating being made to meet long Between heat-resisting high-temperature process, play antiseepage copper facing protective effect.
Technical solution of the present invention: a kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment, including before non-cyanide pre-plating copper Processing, activation protection, non-cyanide pre-plating copper, no cyanogen thicken copper facing pre-treatment, and no cyanogen thickeies copper facing.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, specifically includes the following steps:
1. coppersmith part to be plated is taken, oil removing, washing, activation；When activation, activating solution sulfuric acid content is 130-160g/L, in room Temperature is lower to activate 5-15s；It is put into after carrying out activation protection in activation protection liquid, is directly placed into copper pre-plating slot after workpiece activation；
2. carrying out copper pre-plating to the workpiece in copper pre-plating slot；
3. washing with water, activating, wash with water again the workpiece after step 2. middle copper pre-plating；
4. carrying out thickening copper facing in step 3. treated workpiece is put into thickening plating copper plating tank；
5. machinery works out the copper plate in face after step 4. treated workpiece washing drying, carries out carburizing, seeps Nitrogen, cyaniding and except after Copper treatment, washing drying.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 1. in, when the described oil removing；Oil removing used Content is 30~50g/L of NaOH, Na2CO3·10H2O20~30g/L, Na3PO4·12H2O20~30g/L and waterglass 3~ 5g/L；The oil removing time is 20~60min.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 1. in, the described activation protection liquid is two kinds, One is steel alloy or carbon steel class material activation protection liquid；HEDP is 5~10g/L in such activation protection liquid；Another kind is Stainless steel-like material, such material all need first nickel preplating, activation protection are carried out after nickel preplating, HEDP is 50 in activation protection liquid ~100g/L.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 1. in, it is described that activation guarantor is carried out to workpiece Shield is；Workpiece activates 5~15s of protection at room temperature.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 2. in, the copper pre-plating is；Using cathode Mobile device carries out copper pre-plating, copper pre-plating parameter are as follows: HEDP and Cu2+Mass ratio reaches 14~21, and pH value is 9.5~10.2；Temperature Degree is 30~45 DEG C；Current density is 1.2~1.5A/dm2；Time is 30~60min；Anode annealed state fine copper plate T1, T2；No Dissolubility anode 1Cr18Ni9Ti or 0Cr18Ni9 stainless steel；S yin: S sun=1:1.0~1.5.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 4. in, when carrying out thickening copper facing, plating used HEDP and Cu in liquid2+Mass ratio is 6~14.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, step 4. in, when carrying out thickening copper facing, using pulse Power supply, frequency 10HZ, first stage plating use forward conduction for 90%, 1.5A/dm2, 10%, 1.0A/dm of negative sense conducting2, Time 2h20min；Second stage uses forward conduction 90%, pulsewidth interval 10%, time 2h, 1.2~1.5A/dm2；Third rank Duan Caiyong direct current electrode position, 1.0~1.4A/dm2, time 1h.
The cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment above-mentioned, the coppersmith part to be plated be steel alloy class material or Stainless steel-like material.
Compared with prior art, this electroplating technology enhances plating solution network based on the displacement copper solved the problems, such as in electroplating process Conjunction ability inhibits the displacement copper phenomenon in electroplating process；Reinforce electroplating work procedure control simultaneously, keeps part surface active shape before plating State improves binding force of cladding material comprehensively, so that coating is met heat-resisting high-temperature process for a long time, plays antiseepage copper facing protective effect.
Detailed description of the invention
Fig. 1 is 4Cr14Ni14W2Coating figure after Mo material work piece 50h nitriding heat treatment；
Fig. 2 is 4Cr14Ni14W2Mo material work piece 50h nitriding heat treatment, which is moved back, seeps point without leakage after copper；
Fig. 3 is the sample after " infusion process " checks porosity；
Fig. 4 is 50h nitriding part；
Fig. 5 is that 50h nitriding heat treatment moves back and seeps point without leakage after copper.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but be not intended as to the present invention limit according to According to.
Embodiment 1.
A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment, the present embodiment is to 4Cr14Ni14W2Mo material work piece into Row cyanide-free copper electroplating: specifically includes the following steps:
1. taking coppersmith part to be plated, oil removing, washing, activation, when activation, sulfuric acid content is 150g/L in activating solution, in room temperature Lower activation 10s；It is put into after carrying out activation protection 10s in activation protection liquid, is directly placed into copper pre-plating slot after workpiece activation；It is described Oil removing be；The content of oil removing used is NaOH 40g/L, Na2CO3·10H2O 25g/L、Na3PO4·12H2O 25g/L and water Glass 4g/L；The oil removing time is 40min；The activation protection liquid hold-up is HEDP50~100g/L.
2. carrying out copper pre-plating to the workpiece in copper pre-plating slot；Copper pre-plating parameter are as follows: HEDP and Cu2+Mass ratio reaches 14~ 21, pH value is 9.5~10.2；Temperature is 30~45 DEG C；Current density is 1.2~1.5A/dm2；Time is 30~60min；Sun Pole annealed state fine copper plate T1, T2；Insoluble anode 1Cr18Ni9Ti or 0Cr18Ni9 stainless steel；S yin: S sun=1:1.0~1.5；
3. by step 2. in workpiece after copper pre-plating, wash with water, activation (method with step 1.) washes with water again；
4. carrying out thickening copper facing in step 3. treated workpiece is put into thickening plating copper plating tank；It thickeies used in copper facing HEDP and Cu in electroplate liquid2+Mass ratio is 6~14, and using the pulse power, frequency 10HZ, first stage plating uses positive guide Lead to for 90%, 1.5A/dm2, 10%, 1.0A/dm of negative sense conducting2, time 2h20min；Second stage uses forward conduction 90%, Pulsewidth interval 10%, time 2h, 1.2~1.5A/dm2；Phase III uses direct current electrode position, 1.0~1.4A/dm2, time 1h.
5. machinery works out the copper plate in face after step 4. treated workpiece washing drying, carries out carburizing, seeps Nitrogen, cyaniding and except after Copper treatment, washing drying.
Inventor detects the workpiece obtained after the present embodiment copper facing, (580 DEG C, 50h) heat of through a long time nitriding Processing, coating has no bubbling phenomenon (see Fig. 1) after 50h nitridation heat treatment, and after strip layers of copper, plating piece does not find that leakage seeps point (see figure 2)。
Embodiment 2.
A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment, the present embodiment are to carry out nothing to 12CrNi3A material work piece Cyanogen copper facing: specifically includes the following steps:
1. taking coppersmith part to be plated, oil removing, washing, activation, when activation, sulfuric acid content is 150g/L in activating solution, in room temperature Lower activation 10s；It is put into after carrying out activation protection 10s in activation protection liquid, is directly placed into copper pre-plating slot after workpiece activation；It is described Oil removing be；The content of oil removing used is NaOH 40g/L, Na2CO3·10H2O30g/L、Na3PO4·12H2O 25g/L and water Glass 4g/L；The oil removing time is 40min；The activation protection liquid hold-up is HEDP 5-10g/L；
2. carrying out copper pre-plating to the workpiece in copper pre-plating slot；Copper pre-plating parameter are as follows: HEDP and Cu2+Mass ratio reaches 14~ 21, pH value is 9.5~10.2；Temperature is 30~45 DEG C；Current density is 1.2~1.5A/dm2；Time is 30~60min；Sun Pole annealed state fine copper plate T1, T2；Insoluble anode 1Cr18Ni9Ti or 0Cr18Ni9 stainless steel；S yin: S sun=1:1.0~1.5；
3. washing with water, activating, wash with water again the workpiece after step 2. middle copper pre-plating；
4. carrying out thickening copper facing in step 3. treated workpiece is put into thickening plating copper plating tank；It thickeies used in copper facing HEDP and Cu in electroplate liquid2+Mass ratio is 6~14, and using the pulse power, frequency 10HZ, first stage plating uses positive guide Lead to for 90%, 1.5A/dm2, 10%, 1.0A/dm of negative sense conducting2, time 2h20min；Second stage uses forward conduction 90%, Pulsewidth interval 10%, time 2h, 1.2~1.5A/dm2；Phase III uses direct current electrode position, 1.0~1.4A/dm2, time 1h.
5. machinery works out the copper plate in face after step 4. treated workpiece washing drying, carries out carburizing, seeps Nitrogen, cyaniding and except after Copper treatment, washing drying.
Inventor detects the workpiece obtained after the present embodiment copper facing, plates 30 μm of thickness, and using HB5037, " copper is plated Layer quality inspection " " infusion process " progress ferroxyl test.It is immersed in particular solution (potassium ferricyanide 10g/L, sodium chloride 20g/L) 5min is kept, the blue spot (see Fig. 3) that 2 strips do not occur is observed after taking-up, illustrates that non-cyanide plating layers of copper is fine and close, Porosity meets navigation mark requirement.
Embodiment 3.
A kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment, the present embodiment is to 4Cr14Ni14W2Mo material work piece into Row cyanide-free copper electroplating: specifically includes the following steps:
1. taking coppersmith part to be plated, oil removing, washing, activation, when activation, sulfuric acid content is 150g/L in activating solution, in room temperature Lower activation 10s；It is put into after carrying out activation protection 10s in activation protection liquid, is directly placed into copper pre-plating slot after workpiece activation；It is described Oil removing be；The content of oil removing used is NaOH 50g/L, Na2CO3·10H2O20g/L、Na3PO4·12H2O 30g/L and water Glass 5g/L；The oil removing time is 60min；The activation protection liquid hold-up is HEDP 100g/L.
2. carrying out copper pre-plating to the workpiece in copper pre-plating slot；Copper pre-plating parameter are as follows: HEDP and Cu2+Mass ratio reaches 14~ 21, pH value is 9.5~10.2；Temperature is 30~45 DEG C；Current density is 1.2~1.5A/dm2；Time is 30~60min；Sun Pole annealed state fine copper plate T1, T2；Insoluble anode 1Cr18Ni9Ti or 0Cr18Ni9 stainless steel；S yin: S sun=1:1.0~1.5；
3. washing with water, activating, wash with water again the workpiece after step 2. middle copper pre-plating；
4. carrying out thickening copper facing in step 3. treated workpiece is put into thickening plating copper plating tank；It thickeies used in copper facing HEDP and Cu in electroplate liquid2+Mass ratio is 6~14, and using the pulse power, frequency 10HZ, first stage plating uses positive guide Lead to for 90%, 1.5A/dm2, 10%, 1.0A/dm of negative sense conducting2, time 2h20min；Second stage uses forward conduction 90%, Pulsewidth interval 10%, time 2h, 1.2~1.5A/dm2；Phase III uses direct current electrode position, 1.0~1.4A/dm2, time 1h.
5. machinery works out the copper plate in face after step 4. treated workpiece washing drying, carries out carburizing, seeps Nitrogen, cyaniding and except after Copper treatment, washing drying.
Inventor detects the workpiece obtained after the present embodiment copper facing, and through a long time nitriding (560 DEG C, 30h+580 DEG C, 20h) heat treatment, coating has no bubbling phenomenon (see Fig. 4) that after strip layers of copper, plating piece does not find to leak after 50h nitridation heat treatment It seeps point (see Fig. 5).

Claims (9)

1. a kind of cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment, it is characterised in that: including non-cyanide pre-plating copper pre-treatment, activation Protection, non-cyanide pre-plating copper, no cyanogen thicken copper facing pre-treatment, and no cyanogen thickeies copper facing.
2. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as described in claim 1, it is characterised in that: specifically include following Step:
1. coppersmith part to be plated is taken, oil removing, washing, activation；When activation, activating solution sulfuric acid content is 130-160g/L, at room temperature Activate 5-15s；It is put into after carrying out activation protection in activation protection liquid, is directly placed into copper pre-plating slot after workpiece activation；
2. carrying out copper pre-plating to the workpiece in copper pre-plating slot；
3. washing with water, activating, wash with water again the workpiece after step 2. middle copper pre-plating；
4. carrying out thickening copper facing in step 3. treated workpiece is put into thickening plating copper plating tank；
5. machinery works out the copper plate in face after step 4. treated workpiece washing drying, carburizing, nitriding, cyanogen are carried out Change and except after Copper treatment, washing is dried.
3. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 1. in, institute When the oil removing stated；The content of oil removing used is 30~50g/L of NaOH, Na2CO3·10H2O20~30g/L, Na3PO4·12H2O 3~5g/L of 20~30g/L and waterglass；The oil removing time is 20~60min.
4. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 1. in, institute The activation protection liquid stated is two kinds, and one is steel alloy or carbon steel class material activation protection liquid；In such activation protection liquid HEDP is 5~10g/L；Another kind is stainless steel-like material, such material all needs first nickel preplating, carries out activation guarantor after nickel preplating Shield, it is 50~100g/L that HEDP in liquid is protected in activation.
5. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 1. in, institute State to workpiece carry out activation protection be；Workpiece activates 5~15s of protection at room temperature.
6. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 2. in, institute The copper pre-plating stated is；Copper pre-plating, copper pre-plating parameter are as follows: HEDP and Cu are carried out using cathode moving device2+Mass ratio reaches 14~ 21, pH value is 9.5~10.2；Temperature is 30~45 DEG C；Current density is 1.2~1.5A/dm2；Time is 30~60min；Sun Pole annealed state fine copper plate T1, T2；Insoluble anode 1Cr18Ni9Ti or 0Cr18Ni9 stainless steel；S yin: S sun=1:1.0~1.5.
7. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 4. in, into When row thickeies copper facing, HEDP and Cu in electroplate liquid used2+Mass ratio is 6~14.
8. the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment as claimed in claim 2, it is characterised in that: step 4. in, into When row thickeies copper facing, using the pulse power, frequency 10HZ, first stage plating uses forward conduction for 90%, 1.5A/dm2, 10%, 1.0A/dm is connected in negative sense2, time 2h20min；Second stage uses forward conduction 90%, pulsewidth interval 10%, time 2h, 1.2~1.5A/dm2；Phase III uses direct current electrode position, 1.0~1.4A/dm2, time 1h.
9. such as the cyanide-free copper electroplating technique of high temperature resistant thermo-chemical treatment of any of claims 1-8, it is characterised in that: institute The coppersmith part to be plated stated is steel alloy class material or stainless steel-like material.
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候广库 等: "合金结构钢脉冲防渗镀铜工艺研究", 《电镀与精饰》 *

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CN114505657A (en) * 2022-04-21 2022-05-17 江苏效玄机电科技有限公司 Gas-shielded welding wire high-speed electrochemical copper plating integrated production process and production line

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